CN106518684A - Efficient trimellitate tri C8-C10 preparation method - Google Patents
Efficient trimellitate tri C8-C10 preparation method Download PDFInfo
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- CN106518684A CN106518684A CN201510579871.8A CN201510579871A CN106518684A CN 106518684 A CN106518684 A CN 106518684A CN 201510579871 A CN201510579871 A CN 201510579871A CN 106518684 A CN106518684 A CN 106518684A
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- Prior art keywords
- water
- ester
- preparation
- stirring
- dealcoholysis
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to an efficient trimellitate tri C8-C10 preparation method, which comprises: (1) an esterifying reaction, wherein trimellitic acid, C8-C10 alcohol and concentrated sulfuric acid are poured into a reaction kettle, stirring is performed, heating is performed until a boiling state is achieved, a reaction is performed, the boiling reflux state is maintained, and the water is separated; (2) water washing; (3) alcohol removing; (4) refining; and (5) filtering, wherein the refined mixing liquid is filtered to obtain the trimellitate tri C8-C10 product. According to the present invention, the trimellitate tri C8-C10 preparation method has characteristics of convenient operation, simpleness, easy performing and production efficiency improving, and is suitable for industrial production.
Description
Technical field
The invention belongs to field of organic compound preparation, especially a kind of efficient tri trimellitate
C8-C10Ester is easy, effective preparation method.
Background technology
In industrial production, plastics industry and war production, tri trimellitate C8-C10Ester as
A kind of important organic compounds and heat-resisting, high temperature plasticizer, it is more next with good electrical property
More it is widely applied.Tri trimellitate C8-C10The usual production method of ester is that direct esterification is anti-
Should, the color for obtaining product is yellow, is difficult to sell as product, it is necessary to carry out further essence
System, that is, carry out the refinement treatment step that reduces pressure, the problem that such preparation method is present：1, due to
Need to realize using expensive high-vacuum pump in decompression refinement treatment step, therefore,
The method has that production equipment is more, costly, thus is difficult to reduces cost.2, by
In decompression refinement treatment step be production tri trimellitate C8-C10During ester it is essential and
Very time-consuming production stage, therefore, there is production time length, low production efficiency in the method
Problem, is unfavorable for the raising of Business Economic Benefit.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, inclined benzene three is refined using refining agent
Three C of acid8-C10Ester, there is provided one kind can save equipment investment, reduces cost, shorten production
Time is simultaneously capable of the tri n hexyl trimellitate preparation method of improve production efficiency.
It is to employ the following technical solutions realization that the present invention solves its technical problem：
A kind of efficient tri trimellitate C8-C10The preparation method of ester, it is characterised in that the method
Comprise the following steps：
(1) step of esterification
By trimellitic acid, C8-C10Alcohol, the concentrated sulfuric acid, in input reactor, stirring is heated to
Boiling reaction, keeps boiling reflux state to separate moisture therein.
(2) water-washing step
Water will be added in mixture after esterification, after stirring, stratification is removed
Water layer therein.
(3) dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, tri trimellitate C is obtained8-C10Ester.
(4) purification step
Refining agent will be added in crude product after dealcoholysis, and stirring is refined one hour.
(5) filtration step
Mixed liquor after will be refined is filtered, and obtains tri trimellitate C8-C10Ester product.
Described refining agent is sodium carbonate, magnesium carbonate, activated carbon, magnesium sulfate weight ratio, is pressed
0.5：1：2：1.5 mix；
The weight ratio of described refining agent and trimellitic acid is 0.05 0.1：1；
Described trimellitic acid, C8-C10Alcohol, the weight ratio of the concentrated sulfuric acid is 1：2.56：
0.002—0.005；
Described water is 0.8 with the weight ratio of trimellitic acid：1.
Advantages of the present invention and good effect are：
1st, this tri trimellitate C8-C10The preparation method of ester in purification step, using refined
Agent (sodium carbonate, magnesium carbonate, activated carbon, sulfuric acid magnesium compound), the product colour for obtaining become
Shallow, it is not necessary to which that high vacuum refinement treatment can be used as product sale, prepared product quality is complete
Meet the technical requirements entirely.This preparation method eliminates high vacuum purification step in production,
The input of high-vacuum pump equipment is avoided, therefore, equipment investment has been saved, production cost has been reduced,
Improve the competitiveness of product in market.
2nd, this tri trimellitate C8-C10The refining agent that the preparation method of ester is used be sodium carbonate,
Magnesium carbonate, activated carbon, sulfuric acid magnesium compound, with cheap, it is easy to the characteristics of purchasing.
3rd, this tri trimellitate C8-C10The preparation method of ester have it is easy to operate, it is simple
Facilitate implementation industrialized production, improve production efficiency.
4th, the present invention in process of production, using refining agent (sodium carbonate, magnesium carbonate, activity
Charcoal, sulfuric acid magnesium compound), it is ensured that product quality and long term storage stability, while of the invention
It is simple with realizing, the investment of production equipment the characteristics of easy to operate, has been saved, life has been improve
Produce efficiency.
Specific embodiment
Below by specific embodiment, the present invention is further described：
Embodiment 1
This tri trimellitate C8-C10The preparation method of ester is comprised the following steps：
1. step of esterification
Heater, electricity stirring, thermometer water circulation condenser and water-oil separating are carried to one
Trimellitic acid double centner, C is put into successively in 500 liters of reactors of device8-C10256 kilograms of alcohol,
0.3 kilogram of the concentrated sulfuric acid, under agitation, micro-vacuum, while being heated to boiling reaction, keeps boiling
Reflux state is risen, is constantly separated water into away from oil water separator, until no moisture is generated
Afterwards, stop heating, esterification terminates.
2. water-washing step
Obtain adding 250 kilograms of water in mixed liquor to after esterification, it is after stirring, quiet
Layering is put, water layer therein is removed.
3. dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, tri trimellitate C is obtained8-C10Ester.
4. purification step
Refining agent (sodium carbonate, magnesium carbonate, activated carbon, sulfuric acid is added in the crude product after dealcoholysis
Magnesium compound) 0.5 kilogram, stirring mixing 1 hour.
5. filtration step
Refined mixed liquor is filtered or press filtration, the liquid for obtaining is tri trimellitate C8-C10
Ester finished product, tri trimellitate C8-C10Ester content 99.0%, color are less than No. 2 (iodine colorimetric).
Embodiment 2
The preparation method of this tri n hexyl trimellitate is comprised the following steps：
1. step of esterification
Heater, electricity stirring, thermometer water circulation condenser and water-oil separating are carried to one
Trimellitic acid double centner, C is put into successively in 500 liters of reactors of device8-C10256 kilograms of alcohol,
0.3 kilogram of the concentrated sulfuric acid, under agitation, micro-vacuum, while being heated to boiling reaction, keeps boiling
Reflux state is risen, is constantly separated water into away from oil water separator, until no moisture is generated
Afterwards, stop heating, esterification terminates.
2. water-washing step
Obtain adding 250 kilograms of water in mixed liquor to after esterification, it is after stirring, quiet
Layering is put, water layer therein is removed.
3. dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, tri trimellitate C is obtained8-C10Ester.
4. purification step
Refining agent (sodium carbonate, magnesium carbonate, activated carbon, sulfuric acid is added in the crude product after dealcoholysis
Magnesium compound) 0.6 kilogram, stirring mixing 1 hour.
5. filtration step
Refined mixed liquor is filtered or press filtration, the liquid for obtaining is tri trimellitate C8-C10
Ester finished product, tri trimellitate C8-C10Ester content 99.0%, color are less than No. 2 (iodine colorimetric).
Embodiment 3
The preparation method of this tri n hexyl trimellitate is comprised the following steps：
1. step of esterification
Heater, electricity stirring, thermometer water circulation condenser and water-oil separating are carried to one
Trimellitic acid double centner, C is put into successively in 500 liters of reactors of device8-C10`256 kilogram of alcohol,
0.3 kilogram of the concentrated sulfuric acid, under agitation, micro-vacuum, while being heated to boiling reaction, keeps boiling
Reflux state is risen, is constantly separated water into away from oil water separator, until no moisture is generated
Afterwards, stop heating, esterification terminates.
2. water-washing step
Obtain adding 250 kilograms of water in mixed liquor to after esterification, it is after stirring, quiet
Layering is put, water layer therein is removed.
3. dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, tri trimellitate C is obtained8-C10Ester.
4. purification step
Refining agent (sodium carbonate, magnesium carbonate, activated carbon, sulfuric acid is added in the crude product after dealcoholysis
Magnesium compound) 0.7 kilogram, stirring mixing 1 hour.
5. filtration step
Refined mixed liquor is filtered or press filtration, the liquid for obtaining is tri trimellitate C8-C10
Ester finished product, tri trimellitate C8-C10Ester content 99.0%, color are less than No. 2 (iodine colorimetric).
It is emphasized that example of the present invention is illustrative, rather than it is determinate,
Therefore the present invention is not limited to the embodiment described in specific embodiment, every by this area skill
The other embodiment that art personnel's technology according to the present invention scheme draws, also belongs to the present invention
The scope of protection.
Claims (1)
1. a kind of efficient tri trimellitate C8-C10The preparation method of ester, it is characterised in that：Should
Method is comprised the following steps：
(1) step of esterification
By trimellitic acid, C8-C10Alcohol, the concentrated sulfuric acid, in input reactor, stirring is heated to
Boiling reaction, keeps boiling reflux state to separate moisture therein；
(2) water-washing step
Water will be added in mixture after esterification, after stirring, stratification is removed
Water layer therein；
(3) dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, tri trimellitate C is obtained8-C10Ester；
(4) purification step
Refining agent will be added in crude product after dealcoholysis, and stirring is refined one hour；
(5) filtration step
Mixed liquor after will be refined is filtered, and obtains tri trimellitate C8-C10Ester product；
Described refining agent is sodium carbonate, magnesium carbonate, activated carbon, magnesium sulfate weight ratio, is pressed
0.5：1：2：1.5 mix；
The weight ratio of described refining agent and trimellitic acid is 0.05 0.1：1；
Described trimellitic acid：C8-C10Alcohol：The weight ratio of the concentrated sulfuric acid is 1：2.56：
0.002—0.005；
Described water is 0.8 with the weight ratio of trimellitic acid：1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510579871.8A CN106518684A (en) | 2015-09-11 | 2015-09-11 | Efficient trimellitate tri C8-C10 preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510579871.8A CN106518684A (en) | 2015-09-11 | 2015-09-11 | Efficient trimellitate tri C8-C10 preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106518684A true CN106518684A (en) | 2017-03-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510579871.8A Pending CN106518684A (en) | 2015-09-11 | 2015-09-11 | Efficient trimellitate tri C8-C10 preparation method |
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|---|---|
| CN (1) | CN106518684A (en) |
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2015
- 2015-09-11 CN CN201510579871.8A patent/CN106518684A/en active Pending
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| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170322 |